CN103710772B - Fiber original liquid coloring superfine carbon black aqueous color paste - Google Patents
Fiber original liquid coloring superfine carbon black aqueous color paste Download PDFInfo
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Abstract
The present invention relates to one and be common to acrylic fibers, superfine carbon black aqueous color paste of viscose original liquid coloring and preparation method thereof, this mill base is by modified carbon black, dispersant, organic solvent and deionized water composition, wherein modified carbon black accounts for 15.0 ~ 40.0% of this mill base gross mass, the mass ratio of dispersant and modified carbon black is 0.15:1 ~ 0.3:1, organic solvent accounts for 5.0 ~ 15.0% of this mill base gross mass, surplus is deionized water, wherein modified carbon black by carbon black through 4-anilinesulfonic acid, at least one surface modifier surface modification in stearmide and barbital and obtaining, the consumption of surface modifier is 2.0 ~ 5.0% of carbon black mass, dispersant is the mixture be made up of for 1:2 ~ 1:5 in mass ratio N-dodecyl iminodipropionate and aliphatic amine polyoxyethylene ether.Disclosed fiber original liquid coloring superfine carbon black aqueous color paste have particle diameter little, with the advantage such as spinning solution compatibility is good, can avoid occurring in spinning process blocking the problems such as spinneret orifice, front and back aberration are large.
Description
Technical field
The present invention relates to a kind of preparation method of the superfine carbon black aqueous color paste for acrylic fibers and viscose glue original liquid coloring, belong to fine chemistry industry science and technology field.
Background technology
At present, organic dyestuff is still adopted to be main to the technique that fiber or fabric dye for the fibre staining such as viscose glue, acrylic fibers, in this technique dye require high, energy consumption is large, light fastness is lower, and dyeing course can produce a large amount of waste water, extremely be unfavorable for the expansion of colored fibre industry energy-saving emission reduction work, at the energy with under the social background that water resource is day by day exhausted, environmental protection pressure increases day by day, how avoid the high energy consumption in dyeing process, high pollution is the major issue being related to textile industry existence.
Original liquid coloring is in the spinning solution of chemical fibre, adds colouring agent and carries out the technique that coloured chemical fiber is directly made in spinning.Colored fibre color aberration prepared by this technique is little, light fastness is high, the more important thing is the chemical fibers dyeing link eliminating downstream, to reducing chemical fibers dyeing cost and promoting that the energy-saving and emission-reduction effect of fiber manufacturing is fairly obvious, be the important means solving the problems such as energy consumption is large, seriously polluted in existing chemical fibre coloring process process, there is good development prospect.
Commercial charcoal blacks mainly exists with the state such as agglomerate or aggregation, large and the skewness of particle, after directly adding spinning solution to, larger impact can be produced to the mechanical property of the rheological property of spinning solution and fiber, need pigment and wetting agent, dispersant, the raw materials such as water are through mixing, dispersion, grinding, filter, the techniques such as froth breaking are prepared into the superfine aqueous color sizing of granules of pigments average grain diameter below 1 micron, sterically hindered or the electrostatic repulsion that this technique mainly utilizes dispersant to be formed on charcoal blacks surface realizes the stable dispersion of carbon black in aqueous phase.But original liquid coloring technique is high to the compatibility of aqueous color paste and spinning solution, stability requirement, because once mill base disperses insufficient or occurs flocculation in spinning solution, the generation of granules of pigments agglomeration will be caused, cause the situation occurring blocking spinneret orifice, color differs; The problems such as the equipment cleaning simultaneously brought in order to avoid colour changing and the excessively waste of color fiber, single batch output of colored fibre is often with hundreds of tons of notes, and the long-time compatibility requirements for mill base and spinning solution is very harsh.Therefore how reduce the pigment particle size of original liquid coloring use mill base, improve its stability, strengthen the compatibility of itself and spinning solution, and then reduce it and reunite in spinning solution, block the critical problem that the problems such as spinneret orifice, front and back aberration be large have just become to prepare original liquid coloring use mill base.
For solving the size controlling of the fiber such as acrylic fibers, viscose glue original liquid coloring use mill base, stability, consistency problem with spinning solution, those skilled in the relevant art expand a large amount of research work.Application number is that the Chinese patent of CN02112308.X discloses and uses at least one in naphthalenesulfonate formaldehyde condensation compound, methyl naphthalene sulfonic acid salt formaldehyde condensation products or benzyl naphthalenesulfonate formaldehyde condensation compound as dispersant, the method of the painted use mill base of acrylic fibers prepared by carbon black, phthalocyanine blue, iron oxide or ultramarine pigment stable dispersion, this mill base can be placed at least 30 days and not have obvious layering and coacervation; Application number is that the Chinese patent of CN200910263472.5 then discloses a kind of method using the auxiliary agent such as dispersant, sagging inhibitor to produce the painted black color paste of viscose glue.
Mill base for acrylic fibers, viscose spinning has higher requirement, the average grain diameter of granules of pigments must be less than 1 micron, require high to the storage stability of mill base, complicated components in acrylic fibers, viscose spinning, containing a large amount of electrolyte, and experience strong acid and strong base process, require during spinning can not because of the reunion of granules of pigments in mill base, stick to the place such as pipeline or spinning head and cause spinnability to be deteriorated, spun look silk requires lower aberration, the look silk of different spinning time will be caused to occur aberration significantly because of mill base and the consistency problem of spinning solution.The improvement of paste formula is mainly absorbed in by viscose glue, acrylic fibers original liquid coloring aqueous carbon black mill base prepared by existing method, these mill bases can only be respectively used to acrylic fibers or viscose glue original liquid coloring, do not have a versatility, and because the compatibility of carbon black particle and spinning solution, production equipment are to problems such as the adsorptivities of granules of pigments, still exist particle diameter bigger than normal, easily block the phenomenons such as aberration is large before and after spinning head, spinning, the long-time compatibility of the spinning solution of itself and the fiber such as acrylic fibers, viscose glue still has much room for improvement.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention starts with from carbon blacksurface modification, surface of pigments performance is changed by surface modification, and screen suitable dispersion, disclose a kind of viscose glue, acrylic fiber original liquid coloring general, the preparation method of the superfine carbon black aqueous color paste with high spinnability, effectively can reduce the particle diameter of original liquid coloring aqueous carbon black mill base, promote the spinnability adding fiber stoste after mill base.
The fiber original liquid coloring superfine carbon black aqueous color paste that the present invention discloses is made up of modified carbon black, dispersant, organic solvent and deionized water, wherein said modified carbon black accounts for 15.0 ~ 40.0% of this fiber original liquid coloring superfine carbon black aqueous color paste gross mass, the mass ratio of described dispersant and modified carbon black is 0.15:1 ~ 0.3:1, described organic solvent accounts for 5.0 ~ 15.0% of this fiber original liquid coloring superfine carbon black aqueous color paste gross mass, and surplus is deionized water.
The present invention's modified carbon black used is obtained through surface modifier surface modification by carbon black, this surface modifier is at least one in 4-anilinesulfonic acid, stearmide and barbital, its consumption accounts for 2.0 ~ 5.0% of carbon black mass, and this carbon blacksurface modified technique utilizes above-mentioned surface modifier to change carbon blacksurface performance in carbon blacksurface absorption.In above-mentioned 3 kinds of surface modifiers, 4-anilinesulfonic acid is slightly soluble in cold water, is dissolved in hot water; Stearmide is water insoluble, is slightly soluble in organic solvent under normal temperature, is dissolved in hot ethanol, chloroform; Barbital is dissolved in hot water and ethanol.Utilize the solubility property of above-mentioned surface modifier in different solvents, the technique that two kinds different can be selected respectively: after surface modifier is dissolved in organic solvent, adding carbon black to disperse at least after 20min through dispersion machine with 300 ~ 1000r/min, grind through three-roll grinder again, modified carbon black is obtained finally by filtration and vacuumize, this optimal process ethanol, as organic solvent, for effectively dissolving relevant surfaces modifier, suitably can heat organic solvent to 40 ~ 55 DEG C; Also surface modifier can be dissolved in the hot water of 80 ~ 100 DEG C, add carbon black, to disperse with 300 ~ 1000r/min at least after 20min through dispersion machine, then through three-roll grinder grinding, filter after being down to room temperature, filter cake obtain modified carbon black through vacuumize.In this surface modification technology, industrial conventional vacuum drying process is generally selected in vacuumize, and control temperature is at 30 ~ 80 DEG C, and controlled pressure is at 0.02 ~ 0.08MPa.
The present invention is using N-dodecyl iminodipropionate and aliphatic amine polyoxyethylene ether as dispersant, its mass ratio is 1:2 ~ 1:5, special needs to be pointed out is, N-dodecyl iminodipropionate can not only play peptizaiton, or a kind of well bactericide, the use of this auxiliary agent can avoid the bactericide that extra use is special in mill base; Disclosed fiber original liquid coloring superfine carbon black aqueous color paste selects the organic solvent accounting for this fiber original liquid coloring superfine carbon black aqueous color paste gross mass 5.0 ~ 15.0% to improve moisture retention and the frost resistance of mill base, at least one in preferred ethylene glycol, propylene glycol, diglycol.
The preparation method of disclosed fiber original liquid coloring superfine carbon black aqueous color paste comprises the steps:
A) reserve 10 ~ 20% of deionized water gross mass, use dispersion machine with 500 ~ 800r/min rotating speed dispersion, 15 ~ 20min all the other deionized waters and dispersant, organic solvent, obtain premix;
B) dispersing speed is adjusted to 300 ~ 500r/min, modified carbon black is added in step a) gained premix, under the rotating speed of 1000 ~ 2000r/min, carry out dispersion be not less than 20min, and in dispersion process, add deionized water reserved in step a), obtain premixed water-based carbon black;
C) step b) gained premixed water-based carbon black is ground in horizontal mill, continuously grinding 5 ~ 10 times, then through deaeration, filtration, obtain fiber original liquid coloring superfine carbon black aqueous color paste.In step c), the zirconium oxide bead of horizontal mill abrasive media preferable particle size 0.4mm ~ 0.8mm used or ceramic bead.
The fiber original liquid coloring superfine carbon black aqueous color paste that the present invention discloses, have that particle diameter is little, spinnability is high, the original liquid coloring of viscose glue and wet spinning acrylic fiber can be common to, good with spinning solution compatibility, can avoid blocking in spinning process the problem such as spinneret orifice, front and back aberration be large.
Detailed description of the invention
By the following example, implementation process of the present invention and outstanding advantages can be set forth further, but the present invention is not limited to the following example.
carbon blacksurface modification
Embodiment 1
200g stearmide is added 8kg temperature in the ethanol of about 55 DEG C, dispersion machine is uniformly mixed 30min with 300r/min speed, obtain the ethanolic solution of stearmide, when temperature keeps about 55 DEG C, 4kg carbon black is added the ethanolic solution of this stearmide, 50min is disperseed to obtain the carbon black of about 55 DEG C with 300r/min again, subsequently this carbon black is ground through three-roll grinder, filter after being down to room temperature, by filter cake at 60 DEG C, the vacuum drying chamber inner drying 50min of 0.08MPa, obtain modified carbon black.
Embodiment 2
20g4-anilinesulfonic acid and 20g barbital are added 5kg temperature in the hot water of about 80 DEG C, dispersion machine is uniformly mixed 50min with 500r/min speed, obtain the aqueous solution of 4-anilinesulfonic acid, when temperature keeps about 80 DEG C, 2kg carbon black is added in the aqueous solution of this 4-anilinesulfonic acid, 20min is disperseed to obtain carbon black with 1000r/min again, subsequently this carbon black is ground through three-roll grinder, filter after being down to room temperature, by filter cake at 80 DEG C, the vacuum drying chamber inner drying 50min of 0.02MPa, obtain modified carbon black.
Embodiment 3
60g barbital is added 4kg temperature be in the hot water of 98 DEG C in, dispersion machine is uniformly mixed 30min with 1000r/min speed, obtain the aqueous solution of barbital, when temperature keeps about 98 DEG C, 2kg carbon black is added in the chloroformic solution of this methylaniline, 40min is disperseed to obtain carbon black with 1000r/min again, subsequently this carbon black is ground through three-roll grinder, filter after being down to room temperature, by filter cake at 30 DEG C, the vacuum drying chamber inner drying 50min of 0.02MPa, obtain modified carbon black.
the preparation of superfine carbon black aqueous color paste of fiber original liquid coloring
Modified carbon black prepared by difference Example 1,2,3 and unmodified carbon black, implement component used with embodiment each in table 1 and contrast and prepare fiber original liquid coloring superfine carbon black aqueous color paste, in table 1, modified carbon black prepared by embodiment 1,2,3 is named as modified carbon black 1, modified carbon black 2 and modified carbon black 3 respectively, and each component all accounts for the percentage calculation of fiber original liquid coloring superfine carbon black aqueous color paste gross mass with it.
The preparation process of embodiment 5 ~ 8 and comparative example 9 ~ 12 mill base is: 20% of reserved deionized water gross mass, all the other 80% deionized waters and the component such as dispersant, organic solvent are used dispersion machine with 500 ~ 800r/min rotating speed dispersion, 15 ~ 20min, obtain premix; Dispersing speed is adjusted to 300 ~ 500r/min, modified carbon black is added in premix, under the rotating speed of 1500r/min, carry out dispersion 30min, and in dispersion process, add reserved deionized water, obtain premixed water-based carbon black; This premixed water-based carbon black is ground in horizontal mill, continuously grinding 5 ~ 10 times, again through deaeration, filtration, obtain fiber original liquid coloring superfine carbon black aqueous color paste, wherein, embodiment 5 ~ 6 and comparative example 9 ~ 12 mill base all grind 10 times, and embodiment 7 grinds 8 times, and embodiment 8 grinds 5 times.
The formula composition of table 1. embodiment 5 ~ 8 and comparative example 9 ~ 13 mill base
the superfine carbon black aqueous color paste performance test of fiber original liquid coloring
Particle diameter is tested: the domain size distribution of the fiber original liquid coloring superfine carbon black aqueous color paste prepared with the Zetasizer NanoZs90 type nano particle size of Malvern Instr Ltd. of Britain and zeta potential instrument testing example 5 ~ 8 and comparative example 9 ~ 12, in test result, D50 represents the minimum grain size that the particle of in surveyed particle 50% can pass through, with D100 represent the minimum grain size that all particles can pass through in survey particle, characterize the domain size distribution of pigment particles in mill base with D50 and D100.
Spinnability is tested:
Acrylic fibers original liquid coloring: after the raw material getting fiber original liquid coloring superfine carbon black aqueous color paste prepared by 2kg embodiment 5 ~ 8 and comparative example 9 ~ 12 and Polyacrylonitrile Fiber Spinning Solution composition 40kg respectively mixes, it is carried out spinning by the spinneret orifice in 0.08 millimeter, 30 hole, spinning speed is 15m/min, continuous spinning 12 hours, observes the situation with or without blocking spinneret orifice.
Viscose glue original liquid coloring: after the raw material getting fiber original liquid coloring superfine carbon black aqueous color paste prepared by 2kg embodiment 5 ~ 8 and comparative example 9 ~ 12 and rayon spinning stoste composition 80kg respectively mixes, it is carried out spinning by the spinneret orifice in 0.08 millimeter, 30 hole, spinning speed is 15m/min, continuous spinning 12 hours, observes the situation with or without blocking spinneret orifice.
Spinning chromatism test: objective ranking method and the GB/T8424.3-2001 textile color stability test Colorimetry of testing relative whiteness according to the mensuration general rule of standard GB/T8424.1 textile color stability testing surface color, GB/T8424.2-2001 textile color stability, to in spinnability test process, get acrylic fibers and viscose that spinning starts preparation in 0.5 hour, 10 hours respectively, contrast different time spin the aberration of look silk.
Above-mentioned test result is as shown in table 2.
Table 2. embodiment 5 ~ 8 and comparative example 9 ~ 12 the performance test results
Claims (5)
1. a fiber original liquid coloring superfine carbon black aqueous color paste, is characterized in that: be made up of modified carbon black, dispersant, organic solvent and deionized water, wherein
Described modified carbon black accounts for 15.0 ~ 40.0% of this fiber original liquid coloring superfine carbon black aqueous color paste gross mass,
The mass ratio of described dispersant and modified carbon black is 0.15:1 ~ 0.3:1,
Described organic solvent accounts for 5.0 ~ 15.0% of this fiber original liquid coloring superfine carbon black aqueous color paste gross mass,
Surplus is deionized water;
Wherein said modified carbon black adopts surface modifier to prepare through following step surface modification by carbon black and obtains:
After surface modifier is dissolved in alcohol organic solvent, adds carbon black and to disperse with 300 ~ 1000r/min at least after 20min through dispersion machine, then through three-roll grinder grinding, obtaining modified carbon black finally by filtration and vacuumize;
Or: after surface modifier being dissolved in the hot water of 80 ~ 100 DEG C, add carbon black and to disperse with 300 ~ 1000r/min at least after 20min through dispersion machine, again through three-roll grinder grinding, carry out after being down to room temperature filtering to obtain soot filter cake, this soot filter cake is obtained modified carbon black through vacuumize;
Above-mentioned surface modifier is at least one in 4-anilinesulfonic acid, stearmide and barbital, and its consumption is 2.0 ~ 5.0% of carbon black mass;
Described dispersant is the mixture be made up of for 1:2 ~ 1:5 in mass ratio N-dodecyl iminodipropionate and aliphatic amine polyoxyethylene ether.
2. fiber original liquid coloring superfine carbon black aqueous color paste according to claim 1, is characterized in that: described organic solvent is at least one in ethylene glycol, propylene glycol and diglycol.
3. fiber original liquid coloring superfine carbon black aqueous color paste according to claim 1, is characterized in that: described alcohol organic solvent is ethanol.
4. the preparation method of the fiber original liquid coloring superfine carbon black aqueous color paste according to claim arbitrary in claims 1 to 3, is characterized in that: comprise the steps:
A) reserve 10 ~ 20% of deionized water gross mass, use dispersion machine to be uniformly dispersed all the other deionized waters and dispersant, organic solvent, obtain premix;
B) modified carbon black is added step a) in gained premix, use dispersion machine dispersion to be not less than 20min, and add in dispersion process step a) in reserved deionized water, obtain premixed water-based carbon black;
C) by step b) in gained premixed water-based carbon black grind in horizontal mill, abrasive media is zirconium oxide bead or the ceramic bead of particle diameter 0.4mm ~ 0.8mm, continuously grinding 5 ~ 10 times, then through deaeration, filtration, obtain fiber original liquid coloring superfine carbon black aqueous color paste.
5. the application of the fiber original liquid coloring superfine carbon black aqueous color paste according to claim arbitrary in claims 1 to 3, is characterized in that: described superfine carbon black aqueous color paste is common to the original liquid coloring of viscose glue and wet spinning acrylic fiber.
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| CN104499079B (en) * | 2014-11-27 | 2016-05-25 | 上海聚友化工有限公司 | A kind of original liquid coloring is prepared the method for black polyester fiber |
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| CN106283244B (en) * | 2016-08-26 | 2018-11-23 | 阜宁澳洋科技有限责任公司 | A kind of preparation method for exempting from printing and dyeing black viscose staple fibre |
| CN107044068B (en) * | 2017-03-09 | 2018-09-14 | 华南理工大学 | A kind of colouring method of heavu weights product and its application |
| CN107587204B (en) * | 2017-09-25 | 2020-04-03 | 浙江纳美新材料股份有限公司 | Pigment dispersion for coloring polyimide stock solution and preparation method thereof |
| CN111155187A (en) * | 2020-01-19 | 2020-05-15 | 浙江纳美新材料股份有限公司 | Conductive black water-based color paste for coloring viscose stock solution and preparation method thereof |
| CN112011842A (en) * | 2020-08-31 | 2020-12-01 | 无锡恒诺纺织科技有限公司 | Preparation method of dope-dyed knitted fabric |
| CN112456467B (en) * | 2020-11-19 | 2022-05-31 | 沈阳化工研究院有限公司 | Modified carbon black applied to spinning resin coloring and preparation method thereof |
| CN113122028B (en) * | 2021-03-29 | 2022-05-13 | 苏州大学 | Instant superfine solid block carbon black and preparation method and application thereof |
| CN115821409A (en) * | 2022-10-26 | 2023-03-21 | 赛得利(江苏)纤维有限公司 | Method for improving blackness of stock solution coloring viscose fibers |
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